I surface modified a porous material, but I want to make sure that I modified both surface of the material as well as the pores of the material? I need a method or an analysis to determine if the modification occurred in the pores of the material.
Make the same modification on non-porous surface and analyse both porous and non-porous surfaces with XPS. It is better if you have BET results, also. You will know the surface area of the porous surface. I fyou would have significantly more signal of functional group with XPS, you can conclude that you have modified even in the porous.
you can also make SEM-EDX analysis, which would be a second proof.
Ozcan, you could use AFM or SEM for morphological analysis. Also depends of the "size" of the details, I means, These are micro-pores ?
I agree with C. Alvani. Measuring a complete nitrogen adsorption/desorption isotherm and analysing the evolution of the textural parameters after the functionalization procedures you will be able to notice whether the grafting of the organic molecules occurred in the pores or at the surface. The functionalization is accompanied by a decrease in the pore size diameter and in the total pores volume, If you observe only a decrease of the SBET value , the functionalization is mainly at the surface of the material. .
Hi I previously used ASAP to look at changes in pores on the surface of acid washed powders so, depending on the pore size, ASAP and/or TEM.
I agree with Handan Acar. The SEM-EDX analysis is a best and fast method for surface analysis after modification.
Positron Annihilation Lifetime Spectroscopy (PALS) may help if the pores are under 30 nm in diameter and you are interested in pore size change. With Coincidence Doppler Broadening Spectrometry (CDBS) one may try to see if the pore surface is unchanged compared to the bulk material, however, it is a little bit tricky to resolve the contributions from the pore surface and the bulk and has to be tested.
Depending on the pore size you could also try confocal microscopy. By tagging your functional groups with a dye you can take sectional images and see if you have fluorescence all over the sample.
Initial sample and modified sample should be subjected for imbibition test of wetting fluid.
The rate of imbibition change confirms the change of surface properties.
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